Extraction of anabolic steroids with aqueous-organic mixtures from hexanic solutions

S. Leschev, Y. Pakhadnia, Aliaksandr A. Ahabalayeu, M. Zayats
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Abstract

The extraction of anabolic steroids (1,4-androstadiene-3,17-dione; 17α-methyltestosterone; 19-norethiocholanolone; 4-hydroxytestosterone; 4-androstene-3,17-dione; 5α-androstane-3β,17β-diol; dehydroepiandrosterone; calusterone; clostebol; methandienone; methyldienolone; nandrolone; testosterone; epitestosterone; tibolone; 19-norandrostenedione; 1-methylene-5α-androstan-3α-ol-17-one) by aqueous-organic mixtures from hexane solutions was studied at the temperature (20 ± 1) °C. Based on the experimental data obtained, the partition ratios of anabolic steroids were calculated, which were used to optimise the standard sample preparation procedure in the process of determining the compounds under study in biologically active dietary supplements and specialised sports nutrition. It was found that the most effective and selective extractants from hydrocarbon solutions are water-acetonitrile mixtures containing from 10 to 20 % by volume of water. An extraction technique has been developed for sample preparation of biologically active dietary supplements for subsequent gas chromatographic determination of anabolic steroids in them using a triple quadrupole mass spectrometric detector. The proposed method is characterised by a standard deviation of 10–15 % and a detection limit about 10 μg/kg of biologically active dietary supplements, which makes it possible to reliably determine impurities of prohibited anabolic steroids in them.
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水-有机混合物萃取己烷溶液中的合成代谢类固醇
合成代谢类固醇(1,4-雄甾二烯-3,17-二酮;17α-methyltestosterone;19-norethiocholanolone;4-hydroxytestosterone;4-androstene-3 17-dione;5α-androstane-3β,17β二醇;脱氢表雄酮;calusterone;clostebol;methandienone;methyldienolone;诺龙;睾酮;epitestosterone;tibolone;19-norandrostenedione;在(20±1)℃的温度下,研究了正己烷水溶液中1-亚甲基-5α-雄甾烷-3α-醇-17- 1的有机混合物。根据所得实验数据,计算合成代谢类固醇的分配比,用于优化生物活性膳食补充剂和专业运动营养中所研究化合物的标准样品制备过程。结果表明,从烃类溶液中提取最有效、最具选择性的萃取剂是水体积比为10% ~ 20%的水-乙腈混合物。开发了一种提取技术,用于生物活性膳食补充剂的样品制备,随后使用三重四极杆质谱检测器气相色谱法测定其中的合成代谢类固醇。该方法的标准偏差为10 - 15%,检测限约为10 μg/kg的生物活性膳食补充剂,可以可靠地测定其中禁用合成代谢类固醇的杂质。
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